LC-MS/MS法测定富马酸替诺福韦二吡呋酯中的9-丙烯基腺嘌呤

Determination of 9- propenyladenine in Tenofovir disoproxil fumarate by LC- MS / MS

目的采用LC-MS/MS法测定富马酸替诺福韦二吡呋酯中的9-丙烯基腺嘌呤。方法采用Waters Acquity UPLCBEH C18色谱柱（50 mm×2.1 mm,1.7μm）,流动相为乙腈-0.1%甲酸溶液,梯度洗脱,流速0.3 mL·min^-1,柱温40℃,质谱离子化方式为ESI,正离子模式,多反应监测,9-丙烯基腺嘌呤检测离子质荷比为m/z176.25→136.15,119.16。结果 1.1-215.4 pg 9-丙烯基腺嘌呤与峰面积的线性关系良好（r=0.998）,检出限为0.1 pg,精密度、稳定性试验的RSD均≤1.5%;平均加样回收率为95.5%,RSD=4.58%（n=9）。结论所用方法准确、快速灵敏、专属性强,可用于测定富马酸替诺福韦二吡呋酯中的9-丙烯基腺嘌呤。

OBJECTIVE To establish an LC- MS / MS method for the determination of 9- propenyladenine in Tenofovir disoproxil fumarate. METHORDS The seperation was performed on a Waters Acquity UPLC BEH C18column（ 50 mm × 2. 1 mm,1. 7 μm）with acetonitrile- 0. 1% formic acid as the mobile phase with elution gradient at the flow rate of 0. 3 m L·min- 1,and the column temperature was 40 ℃. The analytes were analyzed by electro- spray ionization（ ESI） in the multiple reaction monitoring mode. The precursors of production transitions of m / z176. 25 →136. 15,119. 16 were used to measure 9- propenyladenine. RESULTS The linearity range was 1. 1- 215. 4 pg（ r = 0. 998）,and the detection limit of 9- propenyladenine was 0. 1 pg. The RSD of precision and stability was all less than 1. 5%. The average recoveries were 95. 5% with the RSD of 4. 58%（ n = 9）. CONCLUSION This method is accurate,rapid,sensitive and selective,and suitable for the determination of 9- propenyladenine in Tenofovir disoproxil fumarate.